Dinitroglycerin and process of making the same.



it freezes, and the like.

UNITED STATES PATENT @FFTCE.

ANTON MIKOLAJCZAK, 01? CASTROP, GERMANY. I I 'DINITROGLYCERIN ANDPROCESS oF rename THE same.

Specification of Letters Patent.

' Patented Aug. 29, ions.

Application filed April 18, 1904.' Serial No. 208,762,

To all whom it may concern:

Be it known that I, ANTON. MIKOLAJCZAK, a subject of the King ofPrussia, German Emperor, residing at Castrop, Westphalia, Germany, haveinvented certain new and useful Improvements .in Dinitroglycerin andProcesses of Making the Same, of which the following is a specification.

According to present practice'in the manufacture of dynamite, carbonite,and other nitroglycerin explosives the necessary nitro glycerin isprepared in the form of trinitrounrealized, and thus the disadvantages,which,

in addition to its many good qualities,-attach to nitroglycerin have hadto be tolerated. These disadvantages consist in the high sensibility ofthe substance against mechanical shocks and heat, in the readiness withwhich They lead to difiiculties both in its manufacture and in itsapplication and are the cause of many accidents.

For the purpose of removing the disadvantages of nitroglycerin a numberof processes have been invented. I may mention here that of mixingnitrobenzol, amyl nitrate, 850. Most of these processes, however, haveproved a total failure, while others have not been employed with realsuccess in practice. In the employment of dinitroglycerin,G3H5(O.N02)2OH, I'have invented a process of manufacturing explosiveswhich oflers great advantages over the processes referred to.

1. Dinitroglycerin is a considerably more stable compound than theextremely unstable blastingoil trinitroglycerin, 03H5(O.NO 2)3. It istherefore much less sensible against mechanical shocks and heat than thelatter. Pure dinitroglycerin does not explode on ignition at all.Byaddinga gradually-increasing percentage of dinitroglycerin totrinitro- 'lycerin the dangerous characteristics of the fatter can bemore and more modified.

,erin contains too little.

2. Dinitroglycerin can be prepared altogether without danger, since anydecomposition accidentally occurring in the course of manufacture, evenin the case ofvery large quantities, does not cause explosion, asnumerous experiments where decomposition has been purposely broughtabout have proved.

3. Dinitroglycerin for all practical purposes maybe considered asuncongealable. Its addition to trinitroglycerin lowers thefreezing-point of the latter to such an extent ,that a mixture of, forinstance, sixty per cent. dinitro and forty per cent. trinitro glycerin'was found to remain perfectly fluid during severe frost, Whilenitroglycerin lixiviated from commercial dynamites, as well as thelatter themselves, froze completely under-the same experimentalconditions.

f 4. By the selection of suitable quantities of dinitroglycerin andordinary blasting-oil an oil can be produced superior to ordinaryblasting oil in explosive power, for n1troglycerin contains more oxygenthan 18 necessary for combustion of the carbonic acid and ofzthehydrogen to water, while dinitroglyc Thus by mixing these two compoundethers a product equalizing these two conditions can be'obtained, whichmay be regarded as an ideal blastingoil and whereby the greatestpossible explosive force is obtained.

5. What has been said in paragraphs 1, 3, and t in respect todinitroglycerin and its mixtures with blasting-oil naturally appliesalso to all'explosives prepared from-the same for shooting and blastingpurposes. In the case of such explosive powders for shooting or militarypurposes there is the-additional advantage that on account of the lowertemperature of the generated gases, which are also much more slowlygenerated, the barrel of the gun is attacked to a much less degree thanin the case of the Well-known nitroglycerin powders.

6. Dinitroglycerin is not only readily soluble in everyproportion innitroglycerin, but by its aid any suitable *mixture of di'and trinitroglycerin can be prepared directly.

7. Dinitroglycerin isjust as'good a solvent and gelatinizing medium forvarious substances (such as nitro-cellulose, xyloidin, 8:0.) as istrinitroglycerin.

The following examples of explosives may be here giveni u. Sixty-one percent. dinitroglycerin, 1. 8

per cent. soluble pyroxylin,thirty per cent. ptassium nitrate, 7.2 percent. wood-meal; total, one hundred per cent.

b. 38.4. per cent. dinitroglycerin, 25.6 per cent. blasting-oil,(trinitroglycerin,) 1.7 per cent. soluble pyroxylin,twentyseven percent. sodium nitrate, 7.3 per cent. wood-meal; total, one hundred percent.

0. Seventeen per cent. dinitroglycerimfiftyeight per cent. blasting-oil,twenty-three per cent. infusorial earth, (kieselguhr,) two per cent.chalk; total, one hundred per cent.

d. Fifty per cent. dinitroglycerin, fortynine per cent. solublepyroxylin, one per cent. diphenylamin; total, one hundred per cent.

0. Twenty per cent. dinitroglycerin, eighty per-cent. soluble pyroxylin;total, one hundred per cent.

' twenty-three per cent. infusorial earth, (kiesel- 'guhr;) total, onehundred per cent.

Forty-one per cent. dinitroglycerin", thirty-four per cent.trinitroglycerin, one per cent. chalk, twenty-four per cent. infusorialearth, (kieselguhr;) total, one hundred per cent.

Z. Fourteen per cent. dinitroglycerin, seventy-eight per cent.trinitroglycerin, eight per cent. soluble pyroxylin; total, one hundredper cent.

m. 12.5 per cent. dinitroglycerin, 62.5 per cent. trinitroglycerin, oneper cent. chalk, twenty-four per cent.- infusorial earth,'(kieselguhr;)total, one hundred per cent.

As an example of my method of manufacturing dinitroglycerin 1 may citethe following: To ten parts, by weight, of glycerin of- 1.262 specificgravity thirty-three parts, by weight, of nitric acid of 1.50 specificgravity are added, preferab y by allowing the nitric acid to slowly flowinto the glycerin while being stirred, (the temperature being keptdown.) The mixture, chiefly mono-nitroglycerin, is now allowed to coolfor some time (it may be several hours) until the mono-nitroglycerin isconverted into dinitroglycerin.

Said conversion may be accelerated by the use of dehydrating salts orthe like, as is well known to those skilled in the art. The entire massis then diluted with about ten parts, by

weight. of cold water and the nitric acid neutralized by a suitableagent until the lyefor example, in case of using carborate of lime forneutralization---has a specific gravity of 1.58. The dinitroglycerinrises therein and can be readily separated, purified, and dried. Anydinitroglycerin which may remain in the lye can be readily removed bymeans of a solvent, such as ether, and obtainedfrom the latter bydistillation. if desired, the mixture of oil and lye deprived of acidcan be treated in the same manner without prior separation, no technicaldifiiculties being presented.

[)initroglycerin is obtained as a colorless oil when the glycerin andthe nitric acid are colorless -that is to say, free from impurities. Itis soluble in water to a large extent, and by reason of this propertycan very well be obtained quite pure -for instance, by fractionalevaporation of the water. The wellknown solvents for nitroglycerin alsoreadily absorb dinitroglycerin. The percentage of nitrogen according tocalculation is 15.38. An actual analysis (nitrometer and organicanalysis) showed the average to be 15.38 per cent.

If mixtures of dinitroglycerin with trinitroglycerin are employed formanufacturing explosives or gunpowder, the dinitrin and trinitrin canfirst be prepared separately and then mixed. It, however, from nitricacid and sulfuric acid a suitable mixture of certain nitrit'yingefliciency or nitration value is made, said mixture may be used forpreparing and obtaining direct a mixture of both the trinitroglycerinand the dinitroglycerin /I. a,

a mixture containing the desired percentage of dinitroglycerin.

()n the percentage of di and tri nitroglycerin in the product, inaddition to the concentration and proportion of the two acids, thetemperature and the duration of nitrification exert an influence, aswell known in the case of nitrifications generally.

With this method of Working, therefore, the separated oil consists of diand tri nitroglycerin. A considerable part of the nitrated glycerinremains dissolved in the waste acid and can by the addition of furthc'racid mixture, concentrated sulfuric acid, or other dehydrating agent beseparated from it in the form of an oil consisting partly or wholly oftrinitroglycerin.

Whatl claim as my invention, and desire to secure by Letters Patent,is-- 1. The process of manufacturing dinitroglycerin which consists inreacting on glycerin with nitric acid, maintaining a low temperatureuntil dinitroglyeerin is formed and neutralizing the excess of acid, asset forth.

2. The process of manufacturing dinitroglycerin which consists inreacting on glycerin with nitric acid, maintaining alow temperatnreuntil-dinitrogiycerin is formed and neu- Lralizing the excess of acid bymeans of an alkaline carbonate.

3. The process of manufacturing dinitrcglycerin Which consists inreacting on glycerin with nitric acid, maintaining a 'low tempera inureuntil dinitroglycerin is formed and. new tralizing the excess of acid bymeans of an! Witnesses:

alkaline-earth carbonate. i

4c. The compound dinitroglyccr n, ancily liquid having the formulaC3H5OH(ONO2)2,

.115; at a lower temperathre and pbssessing a gzeanei' soiubiliey' inWater'than trinitrogiyc= .erinu i M QF in testimony whereof I havea'ifixed my signature in presence of twc Witnesses.

ANTQN MEKOLAJCZAK.

i and beingfurther characterized by solidifyi P3331: MULLER, EMILGALLENBERG.

